11 results about "N-butyl nitrite" patented technology

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazole compound under a visible light catalysis condition. The method comprises the following steps: dissolving a compound 1 in 1, 2-dichloroethane, then adding tert-butyl nitrite, tribromomethane, alkali and a photocatalyst, in an inert gas environment, irradiating with visible light and stirring at room temperature to react, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column purification on a crude product to obtain a product, namely the isoxazole compound. The brand-new method for preparing the isoxazole compound through visible light catalysis is developed, the conditions of high temperature and high pressure in a traditional synthesis method are avoided, energy consumption and environmental pollution are remarkably reduced, and the yield of the isoxazole compound is effectively increased by regulating and controlling reaction conditions and optimizing raw material selection and proportion.

This invention discloses a solution-based synergistic catalytic method for preparing post-functionalized polyolefins, belonging to the field of polymer material modification technology. The method includes the following preparation steps: adding polyolefin, graft monomer, and catalyst to an organic solvent, stirring until homogeneous, and heating to react, thereby obtaining the post-functionalized polyolefin; wherein the catalyst is a combination of a first catalyst and a second catalyst; and the first catalyst is selected from tert-butyl nitrite, and the second catalyst is selected from N-hydroxysuccinimide and / or N-hydroxyphthalimide. This invention utilizes a synergistic catalytic system composed of tert-butyl nitrite and N-hydroxysuccinimide and / or N-hydroxyphthalimide to activate the C-H bonds of polyolefins in an organic solvent via a free radical mechanism, thereby grafting polar functionalized graft monomers onto the main chain of various polyolefins.

The invention provides an aryl alkyl ketoxime derivative as well as a preparation method and application thereof, and relates to the field of aryl oxime derivatives. The preparation method of the aryl alkyl ketoxime derivative comprises the following steps: by taking potassium formate as an additive, carrying out free radical reaction on a compound I and a compound II under ultraviolet irradiation in the presence of tert-butyl nitrite to obtain the aryl alkyl ketoxime derivative, the compound I is substituted iodobenzene or iodopyridine; the compound II is substituted styrene or thienyl ethylene; wherein a hydrogen atom transfer / single electron transfer relay sequence is utilized to activate a compound I, and tert-butyl nitrite is adopted as a bifunctional reagent, and is used as a hydrogen atom transfer reagent and an oxime source. According to the preparation method of the aryl alkyl ketoxime derivative, pre-functionalization is not needed, a reaction substrate is wide in universality and good in compatibility, reaction conditions are mild, operation is easy and convenient, a target product can be efficiently and rapidly prepared on the premise of high yield, and a new way is provided for oxime synthesis.

The invention discloses a method for co-production of 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride, and belongs to the technical field of organic chemical industry, 2, 4-dichlorofluorobenzene is used as a raw material, alkylation and reaction with tert-butyl nitrite are performed to generate oxime, and then hydrochloric acid hydrolysis is performed to generate 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride; according to the method, co-production of the 2, 4-dichloro-5-fluoroacetophenone and the hydroxylamine hydrochloride is innovatively realized, not only are high yield and high purity of the target product 2, 4-dichloro-5-fluoroacetophenone ensured, but also the nitrogen element in the reaction is recycled and converted into the hydroxylamine hydrochloride with high additional value, and the atom economy is remarkably improved; according to the method, the operation process is greatly simplified, the use of dangerous reagents is avoided, and the intrinsic safety and environmental friendliness of the process are improved from the source; the method is simple to operate, safe and environment-friendly, the production cost is effectively reduced, and the market competitiveness of the product is enhanced.

This invention discloses the application of a thiazo[a]thiazolium fluorescent derivative in the sensing and detection of butyl nitrite. This fluorescent derivative uses the electron-deficient thiazo[a]thiazolium group as the core, with symmetrically connected at both ends a benzene ring with a typical "propeller" conformation and methoxylated triphenylamine at the para- or ortho-position as electron donors, forming a D-A-D type structure. This derivative exhibits high fluorescence quantum yield, excellent intramolecular charge transfer (ICT) characteristics, and good photophysical properties, demonstrating excellent sensing performance for butyl nitrite, including high sensitivity, fast response speed, and short recovery time. Furthermore, this fluorescent derivative is prepared into a fluorescent sensing film with good photochemical stability using a drop-coating method, and then assembled into a device to construct a thin-film fluorescent sensor, demonstrating significant application potential and practical value in the high-sensitivity detection of butyl nitrite.

The invention discloses a preparation method of 4, 6-dichloro-5-methoxypyrimidine, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking dimethyl methoxymalonate as a raw material, generating 2-amino-4, 6-dihydroxy-5-methoxypyrimidine from dimethyl methoxymalonate and guanidine salt under the action of sodium ethoxide; then under the action of tert-butyl nitrite, lithium chloride, salicylic acid and tris (pentafluorophenyl) boron, 4, 6-dihydroxy-5-methoxypyrimidine is generated; finally, under the action of phosphorus oxychloride, 4, 6-dichloro-5-methoxypyrimidine is generated. According to the route, in the first step, a 2-aminopyrimidine product is generated through guanidine salt, in the second step, amino is eliminated through azotization, and the synthesis method of the compound is enriched.

This invention discloses a 4-(formaldehyde oxime)-fluoro-2-quinolinone compound and its synthetic method, belonging to the fields of organic synthetic chemistry and medicinal chemistry. Using halogen-containing fluoro-N-(2-vinylphenyl)acetamide compounds as starting materials, this invention utilizes a visible light-induced tandem cyclization reaction to obtain 4-(formaldehyde oxime)-fluoro-2-quinolinone compounds in high yield. This invention employs greener and cleaner visible light as an energy source and uses inexpensive and readily available tert-butyl nitrite and trimethylamine borane as dual-role reagents (hydrogen transfer reagent and oxime source) and halogen atom transfer reagent, respectively, avoiding the use of expensive transition metal catalysts. The raw materials are simple and readily available, the process is environmentally friendly, and the target product yield is high.

The invention belongs to the technical field of preparation of deuterated organic compounds, and particularly relates to a synthetic method of deuterated chlorobenzene-D4, which comprises the following steps: reacting deuterated aniline, benzyltriethylammonium chloride and tert-butyl nitrite to prepare the deuterated chlorobenzene-D4. According to the method, the synthesis process is mild and easy to control, the requirement for equipment is low, the raw materials are low in price and high in utilization rate, and the purity and the deuteration rate of the prepared deuterated chlorobenzene-D4 are high.

The invention relates to a preparation method of a cefixime intermediate, which belongs to the technical field of drug intermediate synthesis, and comprises the following steps: 1, synthesizing an oxime ether intermediate by using tert-butyl acetoacetate as an initial raw material and using a two-step one-pot method; in the second step, a chlorination-cyclization one-pot reaction is adopted, wherein the oxime ether intermediate reacts with NOCl generated by hydrochloric acid and tert-butyl nitrite, and a chlorination product is generated; carrying out cyclization reaction with thiourea and triethylamine to obtain an acid intermediate; and 3, in order to avoid decomposition of the product, respectively pulping the acid intermediates-dichloromethane, DM-triethylamine and triphenylphosphine-dichloromethane, and mixing and reacting in the microchannel to finally obtain the cefixime intermediate. The whole synthesis route avoids strong acid and other raw materials with great environmental pollution, avoids generation of byproducts, obtains high-yield and high-purity products, and shows better economic advantages.

The application discloses a method for preparing post-functionalized polyolefin by melt method and synergistic catalysis, and belongs to the technical field of polymer material modification. m The grafting reaction is carried out, extrusion and cooling are performed, and the post-functionalized polyolefin is obtained; wherein the catalyst is selected from the combination of tert-butyl nitrite and N-hydroxyphthalimide. The application realizes efficient and high-selectivity graft modification of the polyolefin under the melt processing condition by utilizing the synergistic catalysis of tert-butyl nitrite and N-hydroxyphthalimide, effectively inhibits degradation side reactions, and maintains excellent performance of the base material.

This invention relates to the field of organic synthesis technology and discloses a high-yield synthesis method for benzofuran-2,3-dione 3-(O-methyloxime)2-oxime. The method uses o-hydroxyacetophenone as the starting material and includes the following steps: Step 1, the starting material is refluxed with N,N-dimethylformamide dimethyl acetal in an aromatic hydrocarbon solvent to obtain an enamine ketone intermediate; Step 2, the enamine ketone intermediate is nitrosated and oxidatively cyclized using sodium nitrite and tert-butyl nitrite in a ketone solvent; Step 3, the cyclized product is reacted with methoxyamine hydrochloride in an alcohol solvent to obtain the target product. This invention avoids the use of hazardous reagents such as sodium hydride and concentrated nitric acid by constructing an enamine ketone intermediate and employing a mild two-component nitrosation system. The reaction conditions are mild, and post-processing only requires solid-liquid separation. This method has the advantages of high yield, good purity, high safety, and simple operation, making it suitable for industrial production.